Determination of Sulfur in Fly Ash by High Frequency Combustion Infrared Absorption Spectroscopy with Matrix Matching

CAI Weiting; SONG Junpeng; ZHANG Minghui; WANG Anli; RONG Wenna; LI Bei

doi:10.15898/j.ykcs.202412190263

Rock and Mineral Analysis > 2025 > In Press, Accepted Manuscript > DOI: 10.15898/j.ykcs.202412190263

CAI Weiting，SONG Junpeng，ZHANG Minghui，et al. Determination of Sulfur in Fly Ash by High Frequency Combustion Infrared Absorption Spectroscopy with Matrix Matching [J]. Rock and Mineral Analysis，2025，44（4）：1−8. DOI: 10.15898/j.ykcs.202412190263

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Determination of Sulfur in Fly Ash by High Frequency Combustion Infrared Absorption Spectroscopy with Matrix Matching

Tianjin Baogang Research Institute of Rare Earths Co., Ltd., Tianjin 300300, China

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Received Date: December 18, 2024
Revised Date: January 23, 2025
Accepted Date: January 28, 2025
Available Online: February 21, 2025

Abstract

HIGHLIGHTS
(1) In order to avoid matrix effect, and prepare the effective samples, the occurrence state of sulfur in fly ash was studied by SEM-EDS.

(2) Calcium sulfate is added into the fly ash matrix to prepare calibration sample to avoid the deviation caused by the difference of the matrix.

(3) The orthogonal experiment of 4 factors and 3 levels with the flux addition amount and the flux adding order as factors was designed to determine the best experimental scheme.

ABSTRACT

Fly ash can be used as concrete admixture. If the sulfur content in fly ash is too high, the volume of concrete will change, resulting in expansion cracking and other problems. Therefore, accurate determination of sulfur content in fly ash is great significance for the fly ash application. The sulfur content in fly ash is determined by barium sulfate mass method, which has complicated process, complicated operation, strict requirements for personnel and operation. It was found that the sulfur in fly ash was mainly combined with calcium by SEM-EDS. In order to avoid the influence of matrix effect, a synthetic calibration sample was prepared by adding calcium sulfate to the matrix of fly ash sample. The sulfur content in fly ash was determined by high frequency combustion infrared absorption method. In order to explore the best experimental scheme, the orthogonal test with 4 factors and 3 levels was designed. The 4 factors were quality of flux (iron, tungsten, tin), and the adding order of flux and sample. The influence of analysis time, sample weight and other parameters on the determination of sulfur content was also investigated. The calibration curve equation is y=2194.4x+8.21, the correlation coefficient r=0.9998, the detection limit of the method is 0.00036% (mass fraction, the same below), and the limit of quantitation is 0.0012%. The relative standard deviation (RSD) of sulfur content in fly ash is 0.6%-2.1% and the results are consistent with those of barium sulfate mass method. Compared with barium sulfate mass method, this method is simple to operate and can rapidly and accurately determine sulfur content in actual fly ash sample.
- high frequency combustion infrared spectroscopy,
- fly ash,
- sulfur,
- flux,
- sample weight

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References (28)

References

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